EP2411340B1 - Procédé amélioré destiné à la fabrication d'une fibre optique dopée avec un lanthanide au moyen d'un nouveau co-dopant. fibre optique fabriquée avec et utilisation de la fibre - Google Patents
Procédé amélioré destiné à la fabrication d'une fibre optique dopée avec un lanthanide au moyen d'un nouveau co-dopant. fibre optique fabriquée avec et utilisation de la fibre Download PDFInfo
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- EP2411340B1 EP2411340B1 EP10720035.4A EP10720035A EP2411340B1 EP 2411340 B1 EP2411340 B1 EP 2411340B1 EP 10720035 A EP10720035 A EP 10720035A EP 2411340 B1 EP2411340 B1 EP 2411340B1
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims description 76
- 150000002910 rare earth metals Chemical class 0.000 title claims description 53
- 238000000034 method Methods 0.000 title claims description 52
- 239000000835 fiber Substances 0.000 title claims description 48
- 239000013307 optical fiber Substances 0.000 title claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 75
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 45
- 239000010410 layer Substances 0.000 claims description 39
- 239000000377 silicon dioxide Substances 0.000 claims description 34
- -1 RE salt Chemical class 0.000 claims description 27
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 23
- 239000004071 soot Substances 0.000 claims description 23
- 239000012792 core layer Substances 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 17
- 230000008021 deposition Effects 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 229910052681 coesite Inorganic materials 0.000 claims description 13
- 229910052906 cristobalite Inorganic materials 0.000 claims description 13
- 230000018044 dehydration Effects 0.000 claims description 13
- 238000006297 dehydration reaction Methods 0.000 claims description 13
- 229910052682 stishovite Inorganic materials 0.000 claims description 13
- 229910052905 tridymite Inorganic materials 0.000 claims description 13
- 238000005253 cladding Methods 0.000 claims description 11
- 150000002500 ions Chemical class 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- 238000010348 incorporation Methods 0.000 claims description 8
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 230000000994 depressogenic effect Effects 0.000 claims description 5
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 5
- 239000003607 modifier Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims description 4
- 159000000009 barium salts Chemical class 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 150000001805 chlorine compounds Chemical group 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims 2
- 239000002184 metal Substances 0.000 claims 2
- 239000000243 solution Substances 0.000 description 26
- 230000007547 defect Effects 0.000 description 12
- 239000002019 doping agent Substances 0.000 description 12
- 229910052782 aluminium Inorganic materials 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 230000003287 optical effect Effects 0.000 description 9
- 229910052698 phosphorus Inorganic materials 0.000 description 9
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 229910052691 Erbium Inorganic materials 0.000 description 7
- 238000007598 dipping method Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 230000001476 alcoholic effect Effects 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 229910052788 barium Inorganic materials 0.000 description 5
- 229910006113 GeCl4 Inorganic materials 0.000 description 4
- 229910052769 Ytterbium Inorganic materials 0.000 description 4
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000004453 electron probe microanalysis Methods 0.000 description 4
- HDGGAKOVUDZYES-UHFFFAOYSA-K erbium(iii) chloride Chemical compound Cl[Er](Cl)Cl HDGGAKOVUDZYES-UHFFFAOYSA-K 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 description 4
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 3
- 229910001626 barium chloride Inorganic materials 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 229910052732 germanium Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 2
- 150000002123 erbium compounds Chemical class 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 238000007496 glass forming Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910017544 NdCl3 Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001399 aluminium compounds Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000000146 host glass Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- CKLHRQNQYIJFFX-UHFFFAOYSA-K ytterbium(III) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Yb+3] CKLHRQNQYIJFFX-UHFFFAOYSA-K 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
- C03B37/01838—Reactant delivery systems, e.g. reactant deposition burners for delivering and depositing additional reactants as liquids or solutions, e.g. for solution doping of the deposited glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/045—Silica-containing oxide glass compositions
- C03C13/046—Multicomponent glass compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/0071—Compositions for glass with special properties for laserable glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
- C03B2201/28—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with phosphorus
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/31—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with germanium
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/54—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with beryllium, magnesium or alkaline earth metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Definitions
- the present invention relates to an improved method for fabricating rare earth (RE) doped optical fiber using a new codopant.
- RE Rare-earth
- the RE elements doped into the core of such fibers act as the active medium.
- Different REs like Er, Nd, Yb, Sm, Ho and Tm can be doped to get lasing and amplification covering a wide range of wavelengths.
- Er doped fiber amplifier (EDFA) due to its high quantum efficiency and broad gain bandwidth shows tremendous application in communication field meeting up the huge bandwidth requirement in internet services and information technology.
- RE-doped fiber lasers are replacing gas based or solid state lasers in most of the applications due to their compactness, excellent beam quality and easy handling capability.
- Fiber laser devices are suitable for a variety of applications viz. material processing (cutting, grinding and engraving), range finding, medical and military applications.
- material processing cutting, grinding and engraving
- range finding range finding
- medical and military applications
- doped cladding layer with desired thickness is deposited within a high silica glass substrate tube to produce matched clad or depressed clad type structure followed by deposition of core layers of predetermined composition containing index-raising dopant like GeO 2 at a lower temperature to form unsintered porous soot.
- Deposited soot layer is then immersed into an aqueous solution of the dopant precursor (typical concentration 0.1 M) up to 1 hour. Any soluble form of the dopant ion is suitable for preparation of the solution, although rare earth halides have been mostly used. After dipping, the tube is rinsed with acetone and remounted on lathe.
- the core layer containing the RE is then dehydrated and sintered to produce a clear glassy layer.
- Dehydration is carried out at a temperature of 600°C by using chlorine.
- the level of OH - is reduced below 1 ppm using Cl 2 /O 2 ratio of 5:2 provided the drying time exceeds 30 min.
- the tube is collapsed in the usual manner to get a solid glass rod called preform from which fiber is drawn using conventional method.
- the segregation of AlCl 3 in the preform formation process is suppressed due to the presence of phosphorus and as a result the doping concentration of Al ions can be set to a high level (>3 wt%). It has been also claimed that the dopants concentration and component ratio of Er, Al and P ions having extremely accurate and homogeneous in the radial as well as in longitudinal directions.
- Anhydrous AlCl 3 is preferred in order to omit the dehydration step.
- the solution can also be used in the form of a mist in a soot-like core glass by which it becomes possible to control the doping concentration in high accuracy.
- the distribution of the doping concentration along the radial direction of the core can be arbitrarily set by controlling the deposition temperature of soot like core glass.
- the deposited particulate layer is presintered by backward pass with flow of GeCl 4 and/or corresponding dopant halides and is soaked into an alcoholic/aqueous solution of RE-salts containing codopants such as AlCl 3 in definite proportion followed by conventional steps to obtain the final preform.
- the fiber was drawn from preform in a usual method maintaining suitable core-clad dimensions and geometry. Further reference is made to the documents US2002114607 , US2030213268 , and WO03063308 for the use of BaO in optical fibre preform manufacturing.
- the main object of the present invention is to provide a new codopant for fabricating rare earth (RE) doped optical fiber which obviates the drawbacks of the hitherto known prior art as detailed above.
- RE rare earth
- Another object of the present invention is to provide a method where the core-clad interface problem associated with high level of Al doping is eliminated.
- Yet another object of the present invention is to provide a method where the core-clad defect generation is eliminated without any base loss increase in the fibers.
- Still another object of the present invention is to provide a method where the RE concentration uniformity along the preform/fiber length is maintained even for elimination of codopant such as Al used in the known techniques.
- Yet another object of the present invention is to provide a method which produces relatively low optical loss in the 0.6-1.6 ⁇ m wavelength region.
- the present invention provides an improved method for fabricating rare earth (RE) doped optical fiber using a new codopant according to claim 1 comprising the following steps:
- the unsintered core layer deposition temperature is selected within the range of 1200-1300°C preferably in the range of 1250-1280°C.
- the unsintered particulate layer comprises at least one of GeO 2 , P 2 O 5 or other glass forming oxides as refractive index modifiers.
- the thickness of the porous layer ranges from 3 to 25 ⁇ m.
- RE salt used is chloride, or nitrate.
- the source of Barium Oxide is Barium salt selected from chloride or nitrate.
- solution for Barium and RE salts are prepared using water as solvent.
- soaking period is adjusted between 30 and 90 minute, preferably 45 minute.
- the mixture of O 2 and He may be in the range of 3:1 to 6:1 during oxidation.
- the ratio of Cl 2 :O 2 during dehydration ranges from 1.5:1 to 3:1.
- the dehydration period lies between 45 and 90 minute, preferably 60 minute.
- the porous core layer is sintered in presence of O 2 and He gas within temperature range of 1200°C to 1850°C.
- the RE concentration in the fiber core is increased with increasing RE concentration in soaking solution.
- the concentration of RE ion is controlled by adjusting the porosity of the deposited soot layer.
- the core-clad interface is defect free even at high co-dopant concentration.
- the resulting fiber exhibits relatively low optical loss in the 0.6-1.6 ⁇ m wavelength region compared to the fibers fabricated by conventional method.
- compositions of the core and cladding glass can be adjusted to achieve Numerical Aperture (NA) of 0.15 to 0.25 and RE 3+ ion concentration in the range of 100 to 2000 ppm in the ultimate fiber.
- NA Numerical Aperture
- Still another embodiment of the invention provides a rare earth (RE) doped optical fiber prepared by the said process according to claim 1, comprising SiO 2 in the range of 88-90 mol%, GeO 2 in the range of 9-11 mol%, BaO 0.1-0.9 mol%, and rare earth metals selected from Er2O3 and Yb2O3 in the range of 0.01-0.06 mol%.
- RE rare earth
- the novelty of the present invention lies in obtaining optical fibers doped with various concentrations of RE in the preform/fiber core without formation of defect centers which degrades the optical properties of the fibers.
- the Inventive step lies in identification of a new codopant Ba instead of commonly used codopant like Al or Phosphorous.
- the incorporation of Ba-oxide helps to eliminate unwanted core-clad interface problem and achieve relatively low optical loss in the 0.6-1.6 ⁇ m wavelength region thereby improving the reproducibility of the process in producing fibers with desired optical properties.
- the present invention proposes the use of Ba as an alternate codopant which does not have any undesirable absorption or emission peak in silica operating wavelength region and in addition provides, smooth core-clad interface.
- incorporation of Ba changes the refractive Index (RI) difference of core layer appreciably (more than Al) compared to cladding glass and provides the advantage of adjusting the Numerical Aperture (NA).
- RI refractive Index
- NA Numerical Aperture
- the composition of the core and cladding glass are controlled in a manner to achieve NA between 0.15 and 0.25. The modification provides good control over RE incorporation and uniformity along the preform/fiber length comparable to the known techniques.
- the inventive step lies in introducing Ba salt as a new codopant to control the RE incorporation in fabrication of the RE doped optical fiber and provide smooth core-clad interface [ Figure 2 ].
- the inventive step resides in the use of Barium Oxide (BaO) generated from Barium salt in situ as a codopant.
- the core-clad interface is defect free even at high co-dopant concentration.
- Al or P is added to increase the RE solubility in the fiber core since the large RE ions cannot be accommodated within the rigid network of silica due to absence of sufficient non-bridging oxygen.
- the main advantage of introducing Ba as co-dopant is elimination of unwanted defect generation in the form of star-like patterns along the core-clad interface, which are very common in case of high Al-doped fibers, especially Al doped germano-silicate fibers.
- the defect formation is associated with scattering and degradation in optical properties of the fibers.
- a rare earth (RE) doped optical fiber is prepared by implementing the method as defined.
- the optical fiber comprises SiO 2 in the range of 88-90 mol%, GeO 2 in the range of 9-11 mol%, BaO 0.1-0.9 mol%, and rare earth metals selected from Er 2 O 3 and Yb 2 O 3 in the range of 0.01-0.06 mol%.
- the optical fiber is suitable for developing fiber lasers, amplifiers and sensors for different purposes and other devices where such fiber is used.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Optics & Photonics (AREA)
- Physics & Mathematics (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
- Lasers (AREA)
Claims (16)
- Procédé amélioré pour la fabrication de fibres optiques dopées aux terres rares (RE) en utilisant un nouveau co-dopant, comprenant les étapes suivantes :a. dépôt d'un revêtement synthétique pur dopé au SiO2 ou au P2O5-F à l'intérieur d'un tube de substrat en verre de silice pour obtenir une structure de type revêtement adapté ou enfoncé,b. formation d'un cœur en déposant une couche de particules non frittées comprenant au moins un des éléments GeO2 et P2O5 sur une surface du tube à une température comprise entre 1200 et 1300 °C, la couche de particules non frittées étant déposée sous la forme d'une couche de suie poreuse ;c. maintien des concentrations de GeO2 entre 3,0 et 15,0 % en moles dans la couche de cœur ;d. maintien des concentrations de P2O5 entre 0,5 et 1,5 % en moles dans le cœur, lorsqu'il est ajouté au GeO2 ;e. trempage du tube contenant la couche de suie poreuse dans une solution contenant du sel RE dans la plage de concentration de 0,002 M à 0,3 M avec du sel métallique dans la plage de concentration de 0,15 (M) à 2,0 (M) ;f. séchage de la couche de cœur imbibée sous N2 sec ou de n'importe quel gaz inerte à travers le tube pendant 10 à 30 minutes ;g. chauffage progressif du tube en présence de O2 et de He dans la plage de température de 700 à 1100 °C pour effectuer l'oxydation ;h. déshydratation de la couche de cœur à une température comprise entre 800 et 1200 °C et en présence de Cl2 et de O2 ;i. frittage de la couche de cœur en présence d'un mélange de O2 et de He dans la plage de température de 1200 à 1850 °C ;j. écrasement du tube à une température comprise entre 2000 et 2300 °C pour obtenir une préforme ;k. gainage de la préforme avec des tubes de silice de dimensions appropriées ;l. étirage de fibres à partir de la préforme ; ledit procédé étant caractérisé par l'utilisation d'oxyde de baryum (BaO) à partir dudit sel métallique comme co-dopant pour contrôler l'incorporation de RE tout en fabriquant la fibre optique dopée au RE et pour y fournir une interface cœur-gaine lisse.
- Procédé selon la revendication 1, la température de dépôt de la couche de particules non frittées se situant de préférence dans la plage de 1250 à 1280 °C.
- Procédé selon la revendication 1, la couche de particules non frittées comprenant au moins l'un des éléments suivants : GeO2, P2O5 en tant que modificateurs d'indice de réfraction.
- Procédé selon la revendication 1, l'épaisseur de la couche de suie poreuse étant comprise entre 3 et 25 µm.
- Procédé selon la revendication 1, le sel RE étant choisi parmi le chlorure ou le nitrate.
- Procédé selon la revendication 1, la source d'oxyde de baryum étant le sel de baryum choisi parmi le chlorure ou le nitrate utilisé pour préparer la solution utilisée dans le procédé.
- Procédé selon la revendication 1, la solution étant préparée à partir d'un solvant choisi parmi l'eau.
- Procédé selon la revendication 1, le temps de trempage utilisé étant de 30 minutes à 90 minutes, mais de préférence 45 minutes.
- Procédé selon la revendication 1, le mélange de O2 et de He pouvant être dans la gamme de 3:1 à 6:1 pendant l'oxydation.
- Procédé selon la revendication 1, le rapport de Cl2:O2 pendant la déshydratation se situant dans la gamme de 1,5:1 à 3:1.
- Procédé selon la revendication 1, la période de déshydratation se situant entre 45 min et 1,5 heure.
- Procédé selon la revendication 1, le frittage ayant lieu en présence de O2 et He à une température comprise entre 1200 °C et 1850 °C.
- Procédé selon la revendication 1, les compositions du cœur et de la gaine étant appropriées pour obtenir une ouverture numérique (NA) comprise entre 0,15 et 0,25.
- Procédé dans lequel la concentration en ions RE3+ est maintenue dans la plage de 100 à 2000 ppm dans la fibre finale.
- Fibre optique dopée aux terres rares (RE) préparée par le procédé selon la revendication 1, comprenant SiO2 dans la gamme de 88 à 90 % en moles, GeO2 dans la gamme de 9 à 11 % en moles, BaO dans la gamme de 0,1 à 0,9 % en moles, et des métaux de terres rares choisis parmi Er2O3 et Yb2O3 dans la gamme de 0,01 à 0,06 % en moles.
- Utilisation d'une fibre optique dopée au RE selon la revendication 15, dans des lasers à fibre, des amplificateurs et des capteurs, pour différents usages et dans d'autres dispositifs où une telle fibre est utilisée.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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IN609DE2009 | 2009-03-27 | ||
PCT/IN2010/000201 WO2010109494A2 (fr) | 2009-03-27 | 2010-03-29 | Procédé amélioré destiné à la fabrication d'une fibre optique dopée avec un lanthanide au moyen d'un nouveau co-dopant |
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EP2411340A2 EP2411340A2 (fr) | 2012-02-01 |
EP2411340B1 true EP2411340B1 (fr) | 2020-12-09 |
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EP10720035.4A Active EP2411340B1 (fr) | 2009-03-27 | 2010-03-29 | Procédé amélioré destiné à la fabrication d'une fibre optique dopée avec un lanthanide au moyen d'un nouveau co-dopant. fibre optique fabriquée avec et utilisation de la fibre |
Country Status (4)
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US (1) | US8649650B2 (fr) |
EP (1) | EP2411340B1 (fr) |
CN (1) | CN102421715A (fr) |
WO (1) | WO2010109494A2 (fr) |
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EP2411340B1 (fr) * | 2009-03-27 | 2020-12-09 | Council of Scientific & Industrial Research | Procédé amélioré destiné à la fabrication d'une fibre optique dopée avec un lanthanide au moyen d'un nouveau co-dopant. fibre optique fabriquée avec et utilisation de la fibre |
EP2495589A1 (fr) | 2011-03-04 | 2012-09-05 | Draka Comteq B.V. | Fibre optique d'amplification dopée par des terres rares pour dispositifs compacts et procédé de fabrication correspondant |
SI3001834T1 (en) * | 2013-05-03 | 2018-07-31 | Council Of Scientific & Industrial Research | PRODUCT PROCESS WITH YTTERBIUM DOPEED OPTICAL FIBER |
GB201711849D0 (en) * | 2017-07-24 | 2017-09-06 | Nkt Photonics As | Reducing light-induced loss in optical fibre |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003063308A1 (fr) * | 2002-01-24 | 2003-07-31 | Np Photonics, Inc. | Lasers a fibre a mode unique en verre phosphate dopee aux terres rares |
US20030213268A1 (en) * | 2002-05-20 | 2003-11-20 | Homa Daniel Scott | Process for solution-doping of optical fiber preforms |
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US5284500A (en) * | 1989-10-31 | 1994-02-08 | Fujitsu Limited | Process for fabricating an optical fiber preform |
JP2766420B2 (ja) * | 1992-04-07 | 1998-06-18 | 株式会社フジクラ | エルビウム添加石英の製造方法 |
US6587633B2 (en) * | 2000-03-30 | 2003-07-01 | Corning Oti, Inc. | Active optical fibre doped with rare earth elements |
US6751990B2 (en) * | 2001-03-06 | 2004-06-22 | Council Of Scientific And Industrial Research | Process for making rare earth doped optical fiber |
DE60117161D1 (de) * | 2001-10-18 | 2006-04-20 | Council Scient Ind Res | Verfahren zur herstellung einer mit seltenen erden dotierten optischen faser |
US6851281B2 (en) * | 2002-03-28 | 2005-02-08 | Council Of Scientific And Industrial Research | Method of fabricating rare earth doped optical fibre |
US7292766B2 (en) * | 2003-04-28 | 2007-11-06 | 3M Innovative Properties Company | Use of glasses containing rare earth oxide, alumina, and zirconia and dopant in optical waveguides |
BRPI0418833B1 (pt) * | 2004-05-11 | 2013-03-19 | composiÇço de vidro de germanato para amplificaÇço de fibra àptica, fibra de amplificador àptico, amplificador àptico, e, dispositivo laser. | |
US7116472B2 (en) * | 2005-02-18 | 2006-10-03 | Fitel Usa Corp. | Rare-earth-doped optical fiber having core co-doped with fluorine |
EP2411340B1 (fr) * | 2009-03-27 | 2020-12-09 | Council of Scientific & Industrial Research | Procédé amélioré destiné à la fabrication d'une fibre optique dopée avec un lanthanide au moyen d'un nouveau co-dopant. fibre optique fabriquée avec et utilisation de la fibre |
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- 2010-03-29 EP EP10720035.4A patent/EP2411340B1/fr active Active
- 2010-03-29 US US13/260,415 patent/US8649650B2/en active Active
- 2010-03-29 WO PCT/IN2010/000201 patent/WO2010109494A2/fr active Application Filing
- 2010-03-29 CN CN2010800190684A patent/CN102421715A/zh active Pending
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Publication number | Priority date | Publication date | Assignee | Title |
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WO2003063308A1 (fr) * | 2002-01-24 | 2003-07-31 | Np Photonics, Inc. | Lasers a fibre a mode unique en verre phosphate dopee aux terres rares |
US20030213268A1 (en) * | 2002-05-20 | 2003-11-20 | Homa Daniel Scott | Process for solution-doping of optical fiber preforms |
Also Published As
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US8649650B2 (en) | 2014-02-11 |
WO2010109494A3 (fr) | 2010-12-09 |
US20120201504A1 (en) | 2012-08-09 |
CN102421715A (zh) | 2012-04-18 |
EP2411340A2 (fr) | 2012-02-01 |
WO2010109494A2 (fr) | 2010-09-30 |
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